Refining of vegetable wax powder



fiatented Aug. 5, 1952 Edward A; Wilderand Elbert s. McLoucl, Racine, S. C. Johnson 8: Son, Inc.,

. Wis., assignors to ."Racinawis'g' x j t 7. in

"This invention relates to the manufacture of raw' imaterial-wax. More specifically, it relates to an improved process I I matter from crude'vegetablew'ax powder;

Many vegetable waxes 'suchf as espartograss wax, carnauba wax and ouricury wax are removed from the plants by mechanical means and are; therefore, in the form of crude wax powder containing small particles of; crude wax f together with particles of other vegetable matter. In the case of carnauba :wax, the leaves are-cutfrom the carnauba palm'and allowed to dry. The wax largely remains inclosed in the crevices ofthe'dry and shrunken. leaves. I When; I I removedirom the leaves, a l arge amount: of leafy matterj becomes mingledfwith the wax particles. This leafy'matter is'falso "in powdered form of a particle size, shape'an'd mass comparableto' that o'fflthewaxpowder from which it cansca'rcely be distinguished. Y i

I Various methods have been proposediorj the 're'moval of this leafy matter or borra as it is known in Brazil. One. of the most successful of these methods, which is nowin commercial use, is that described in U. S; patent toJohnson, Steinle and Gardiner No. 2,275,630; By 'this method the' crude vegetable wax powder is screened through one 'or more screens of about 40"to' 60 mesh, and the fines of the screening operation, which contain thewax, are subjected to a further treatment in a centrifugal'ai'r flotation separator whereby additional leafy matter or borra may be reduced-from its original content of 20-35% down to aminimum of 12%. I Although the above process has contributed considerably toj'the production of light-colored wax, neverthelessithe amount of leafy matter or borra which remains tends to darken the wax fupon subsequent melting. I

I In co-pending application, Serial Number 27,354, now Patent No, 2,527,481, a process is desci'ibed'for purifying crude'carnauba' wax powder by means of a liquid flotationsystem. Now in accordance with our invention, we have .developed an improved process for removing leafy matter or borra from crude vegetable wax powder. This'procesawhich is limited to the treatment of crude vegetable wax powder which has not been melted in the production thereof, comprises contacting. crude vegetable wax powder with water, agitating the wax-water mixture sufficiently to wet the wax, and distribute the wet wax throughout the wax-water mixture,

then agitating the wax layer, as it forms on the surface of the water, at a rate sufficient to prefor removingknownwaxy the 'wax powder is v i A pucatibnivltay 1 5, 194s,- I Serial No. 21,353 I 5 Claims; (01. 209-473) wax from the'wax layer.

nature and purpose of this invention,

same. In theexamplesthe ingredients are given in parts by weight thoroughly wet-with 520 parts of water'with aid the surface of .tiofn-ii'n'. agitation allowsv the" borra"ftoj,-Idescend 'fe'asily tofthe' bottom of the. vessel andfdoes not disturb 'the{ bo'r'ra already settled? T Agitation I is pontiplledlatYthe surfaceIwith theagitate "r'osspieceemoving at' 20 feet per. minute, thereby pre- I vent the ientrapping of borra within: the struc ture of the wax layer,'and recovering powde df having indicatedin a generalrwaylhef the -f0110Wi- 1 ing examples will illustrate'the invention. It is to be understood, however, that such examples are presented merely as illustration of the invention and are not to beconstrued as'limiting'the Now,

unless otherwisefindicated.

I Example 1 Two hundred parts of crude carnau a wax powder," prepared by the method describedfin U. S.1'Patent No. 2,275,630 andcontaining "about 15-18%"0f leafy matter or borra; was charged into;- an open vessel. The wax p wde -was of agitation. After the wax hadbeen thoroughly wet, liquid slurry was formed by placing uiewax water'mixture in a vesselbontain-ing 1560 parts of water. I Carefully controlledagitation-was then commenced, the paddle o r cross pieceofthe agitator having been positioned inthe'slurry at-a distance. about two-thirds the 'depth offlslurry from the top of the liquid surface. "In this posi tion the agitator should be, moved at appro mately feet per minute, average linear sp'e for approximately 10 the sl -.51T 'me he i afae tator isthenslowly elevated andits speed gradually reduced so' thatwhen 'agitaton'crosspiece reaches the ,surface'joi the liquid; slurry about a half hour later, it should be moving at a linear speedpf'. about.20 feet per, minute. Thisvreduc- Yen n th wax; la r gm I h en 'e s t lock parti les of borra withingthe thicker 1e i l e A t o n ou of. s i hws jace, eitat ion, the wax layer is; removed and placed in a permeab b sk t c t u Aft t minutes of centrifugal filtration, -WhlGhf-Iffidlld themoisture content ofthe wax from about to 40%, the wax was broken up into small lumps and ai r -dried inopen trays.

The borra content of he uli ee i w r pew es red ess t about 2% ,was...=continued .as described in Ex mple. l.

Example 2 Example 1 was repeated but before the resulting wax layer was removed, the liquid slurry was allowed to stand quiescent, without agitation, for about an hour. Less wax particles, remained suspended in the intermediate zone between the borra and the surface wax layer thanin-Example 1. After the wax layer was removed and treated as in Example 1, no appreciable diiference 015.1

borra content in the dry wax powder. was ,found over the amount shown in Example 1;

Example: ,3-

Two hundred parts of crude carnauba wax powder, prepared by the method disclosed in U. S. Patent No. 2,275,630 15-18% 'bestarted somewhere in thelovver half of the liquid slurry and maintained for aninitial period of to 12 minutes in such position. For this initial agitation the crosspiece should be moving a at 50 to '70,feet per minute, linear speed, to produce the best results. This speed, as well as the '-2Q-; ieet; .per, minute recommended for surface agitation:;may be varied, depending upon the size and containingyabeutv l of leafy matter or borra, was charged into an open vessel containing 2080-1 partsof water. The crude waxr powder was thoroughly -wet byamechanical agitation and; such agi atio :T resulting wax-layer was removed-and; treat-ed as am Example .1.2The,borra-:contentmftheresult- --ingldryewax powder; was-reduced to about 2 I i In theaabove examples there ,has,-b,een;;;illusrtriated. ouri;improyed process fOrremQYi g-E'I MY matteror .borra'irom; crude vegetable, wax powder; :viThelexamplesgillustrate' the treatment; of dry-crude tvegetable. waxepowderthavin a. a r content; of ':15+18.%., which; upon; treatment was reduced to approximately 2% by the employment of controlled agitation as described.

The wetting of the surface of, the dry crude .-v.egetable ithput i -39:- 3 1 H ered to xpremix thedry cr.ude,yegetable wax pewder, with at least 2. -tiz nes itsweight of water -ard-then;-r eh ei 1pm? eparatilon ofthe borra vcan take showninExamples land 2, itispres .iaohieved, .However, as p163, if desired, the wax may i a larger body of water, ,but n thatthawaxis.added,on1y I at it;- ean-;be.thoroughly wet as it '99QQ 1:.i Q;$ -:Y

If wa i n eaed an vess W th u beamin ile x Wit c t, wi 5ie;un e-i eren -b qu d-lan eien en ra on-1 f.- berm-fem d carrying, out this flpro,cess, cold 'of'a; temperature of about-20,25 The useof hot Water'or'water s mem sg su ns-mleni l ion [of the wax, in thewater and-interferes ii-1e efiicie -eena a m L t ab ra re wax. Thereforegthe use of watenofja .tem-

ature of not more than 70? C..fis recommended. ,hilerinptheqexamples the total volume of irlaterr mva s,.abq1 ..'10: bazea ized tth sra qm y be ya ie While it is recommended .that approximately parts ater tolpart Inthe examples,--the agitatorcrosspiecewas employed in a position two-thirds theidepth of the slurry for approximately 10 minutes and-was ,a itate the mixture, until .v we t it s oul W W of; wax by weight'be used: the ratioofgwater to-wax may be increased over that amount, but the addition of excessive amounts of C5 to use a rotating and type'ofiragitator used.

Various typesand sizes of agitator crosspieces maybe employed, but we have found it expedient rake-like agitator. The action. given the slurry by the projecting teeth of this type of agitator ,prevents the from ;.pa ki; e i h vb thickenips xc ssive y- ;I {he-, structure I or .type of -;agitator; is, chosento accomplish its, purpose while creating a. minimum of turbulence in; the slurry. 1 If desired, 1;iquid up ,a d-e s s s be :us d f -acco plish the "same agitation.

While a the examples have il1ustrated,the.,separation of ,leafy -.carnauba wax powder, itwill be-understood that this process is equally,, applicable to}, other vegetable-wax powders such asaspartcr grass wax, and ouricury wax ,which are. obtained,..from

the commercial uses of thevegetablewax. It ,is 1

anticipated that thedry vegetableawaxrpowder .will be treated .with adsorbents and meltedhthus obtaining a wax of sufficienttlightness to, eliminate the,.necessity .j.of bleaching withchemicals Whichare well known. in theart. While chemical bleachi -(agents ,often, provide a ;lishtness. ,pf color; the ..resulting alteration, of the structural and gchemical, nature; or tn originarwax. is det- .rimental .where the particular char cteri tics of the originalwaxaredesired.

:We claim:

La processrorpurifyin .c udeve etablewa EQWdeIZ w i .Anotibeen.me1ted ,in; tne ro duction thereof, comprising contacting fqrude vegetable wax powder with. w;aterfin a, suita b1e s lv i sbeins' oi. (temperature oi-not ,more thaniml latheat o.b tweemsa d; waxand Water. be n -"at least 2. /2 par s water-l n e-pa of waig agitating the wax-,-water ,niixturegat a .pointgsubstantially below the suriace of, said mixture, and ,in a. manner. sufilcient tor'wet said .wax ,and ;dis tri bute saidawaxlthroughqut 1 .the finti-re yessel.br n in he-a i at amediar e.the :sn fac :;o t rm xtur iwwhile s multane us gradually; reducin athexspeedi her ctra itatin 5 13119.: wax 18131911 35 itiformsvv on:the z surfaceof' sajd :mixture at. a rate .lessvthan halirthat employed in said below-surface f agitation; :said :rate being -sufficient to prevent =entrapping of borra-within the structure of said Way-dayer, recovering "powdered waxfrom saidwax layer.

wax layer matter 1 or borra from,- crude 2. A process for purifying crude carnauba wax powder which has not been melted in the production thereof, comprising contacting crude carnauba wax powder with water in a suitable vessel, said water being of a temperature of not more than 70 C., the ratio between said wax and water being at least 2 parts of water per part of wax, agitating the wax-water mixture at a point substantially below the surface of said mixture and in a manner sufficient to wet said wax and distribute said tire vessel, bringing the agitating media to the surface of the mixture while simultaneously gradually reducing the speed thereof, agitating the wax layer as it forms on the surface of said mixture at a rate less than half that employed in said below-surface agitation, said rate being sufficient to prevent entrapping of borra within the structure of said wax layer, recovering powdered wax from said wax layer.

3. A process for purifying crude vegetable wax powder which has not been melted in 'the production thereof, comprising contacting crude vegetable wax powder with water in a suitable vessel, said water being of a temperature of not more than 70 C., the ratio between said wax and water being at least 2 parts of water per part of wax, increasing the amount of water in said mixture until a liquid slurry is formed, agitating said slurry at a point substantially below the surface of said slurry in a manner to distribute said wax throughout the entire vessel, bringing the agitating media to the surface of the mixture while simultaneously gradually reducing the speed thereof, agitating the wax layer as it forms on the surface of said mixture at a rate less than half that employed in said belowsurface agitation, said rate being sufficient to prevent entrapping of borra within the structure of said wax layer, recovering powdered wax from said wax layer.

wax throughout the enpart of wax, agitating 4. A process for purifying crude carnauba wax I powder which has not been melted in the production thereof, comprising contacting crude carnauba wax powder with water in a suitable vessel, said water being of a temperature of not more than 70 C., the ratio between said wax and water being atleast 2 /2 of wax, increasing the amount of water in said mixture until a liquid slurry is formed, agitating said slurry at a point substantially below the surface of said slurry in a manner to distribute parts of water per part said wax throughout the entire vessel, bringing the agitating media to the surface of the mixture while simultaneously gradually reducing the speed thereof, agitating the wax layer as it forms on the surface of said mixture at a rate less than half that employed in said below-surface agitation agitation, said rate being sufficient to prevent entrapping of. borra within the structure of said wax layer, recovering powdered wax from said wax layer. I 5. A process for purifying crude vegetable wax powder which has not been melted in the production thereof, comprising contacting crude vegetable wax powder with water in a suitable vessel, said water being of a temperature of not more than C., the ratio between said wax and water being at least 2 parts of water per the wax-water mixture at a point substantially below the surface of said mixture and in a manner sufficient to wet said wax and distribute said wax throughout the entire vessel, bringing the agitating media to the surface of the mixture while simultaneously gradually reducing the speed thereof, agitating the wax layer as it forms on the surface of said mixture at arate less than half that employed in said below-surface agitation, said rate being sufficient, to prevent entrapping of borra within the structure of said wax layer, allowing said mixture to remain quiescent until a firmer wax layer is formed on the surface of said water, re covering powdered wax from said wax layer.

EDWARD A. WILDER. ELBERT S. McLOUD.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS OTHER REFERENCES Bennett-Commercial Waxes (1944), Chem. Pub. Company, pages 74 to 76. 

1. A PROCESS FOR PURIFYING CRUDE VEGETABLE WAX POWDER WHICH HAS NOT BEEN MELTED IN THE PRODUCTION THEREOF, COMPRISING CONTACTING CRUDE VEGETABLE WAX POWDER WITH WATER IN A SUITABLE VESSEL, SAID WATER BEING OF A TEMPERATURE OF NOT MORE THAN 70* C., THE RATIO BETWEEN SAID WAX AND WATER BEING AT LEAST 21/2 PARTS OF WATER PER PART OF WAX, AGITATING THE WAX-WATER MIXTURE AT A POINT SUBSTANTIALLY BELOW THE SURFACE OF SAID MIXTURE AND IN A MANNER SUFFICIENT TO WET SAID WAX AND DISTRIBUTE SAID WAX THROUGHOUT THE ENTIRE VESSEL, BRINGING THE AGITATING MEDIA TO THE SURFACE OF THE MIXTURE, WHILE SIMULTANEOUSLY GRADUALLY REDUCING THE SPEED THEREOF AGITATING THE WAX LAYER AS IT FORMS ON THE SURFACE OF SAID MIXTURE AT A RATE LESS THAN HALF THAT EMPLOYED IN SAID BELOW-SURFACE AGITATION, SAID RATE BEING THE STRUCTURE OF SAID WAY LAYER, RECOVERING POWDERED WAX FROM SAID WAX LAYER. 